CN107130231A - Nanometer metallic silver coats the preparation method of synthetic fluoromica powder - Google Patents
Nanometer metallic silver coats the preparation method of synthetic fluoromica powder Download PDFInfo
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- CN107130231A CN107130231A CN201710534173.5A CN201710534173A CN107130231A CN 107130231 A CN107130231 A CN 107130231A CN 201710534173 A CN201710534173 A CN 201710534173A CN 107130231 A CN107130231 A CN 107130231A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/22—Roughening, e.g. by etching
- C23C18/24—Roughening, e.g. by etching using acid aqueous solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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Abstract
A kind of nanometer metallic silver coats the preparation method of synthetic fluoromica powder, comprises the steps：（1）The pretreatment of synthetic fluoromica powder, including：（1‑1）Roughening；（1‑2）Activation, first coats the first active layer, the chemical composition of the first active layer is SnO with liquid-phase precipitation method on roughened synthetic fluoromica powder2、SiO2Or ZnO；Coat the second active layer on the first active layer with liquid-phase precipitation method again, the chemical composition of the second active layer is TiO2、CaO、Al2O3Or ZrO2；（2）Prepare silver ammino solution；（3）By silver mirror reaction, nano metal silver layer is coated on activated synthetic fluoromica powder.The nanometer metallic silver produced by the present invention cladding synthetic fluoromica powder premium properties such as have good conductive and heat-conductive catalytic performance, excellent decoration performance, high intensity, high tenacity, good chemical resistance, nontoxic free from admixture, quality light, and it is with low cost, cost performance is high.
Description
Technical field
The present invention relates to the manufacture of powder, and in particular to a kind of nanometer metallic silver coats the system of synthetic fluoromica powder
Preparation Method.
Background technology
The conductive good, oxidation resistance of silver powder is strong, stable chemical performance the advantages of, but its is expensive, limits
Its extensive use.Rise with the price of international argent, low cost becomes extravagant hope using silver powder.How argent is reduced
Usage amount, to reduce cost, the big problem as puzzlement the sector development.
Commonly powder surface is silver-plated saves silver-colored consumption, if Surface coating can be replaced in any case than more complete
Silver powder.Silver-plated to have plating, chemical plating, vapour deposition process etc. to plant multi-method, wherein chemical plating method has that technique is simple, matrix material
Material should not derivation electricity, suitable for irregular matrix material, cost is relatively low the advantages of, and chemical deposit has high-compactness, thickness
The performance such as homogeneous, the good corrosion resistance of degree and wear resistance, therefore, the metal of powder body material is realized by the method for chemical plating
Change, it has also become the study hotspot of the sector.
There is the silver powder prepared using non-metallic matrix material in present market（The non-metallic powder of electroplate）It is used as
Conductive filler, has the advantages that light weight, electrical and thermal conductivity are good, but technical matters is immature, so that the silver powder prepared is deposited
The problems such as impurity content is big, covering amount is few, clad is more crisp, clad is shaky；And use metal matrix material（Such as copper）
The silver powder of preparation, although quality will generally get well, but price still remains high, and quality weight.Therefore, how one is obtained
The high silver powder of kind of function admirable, with low cost, cost performance, it has also become the problem of urgent need to resolve.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of nanometer metallic silver cladding synthetic fluoromica powder
Preparation method, obtained nanometer metallic silver cladding synthetic fluoromica powder function admirable, with low cost in this way,
Cost performance is high.The technical scheme of use is as follows：
A kind of nanometer metallic silver coats the preparation method of synthetic fluoromica powder, it is characterised in that comprise the steps：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）Take 100 parts by weight synthetic fluoromica powder（By dry weight）, being added to 320-480 parts by weight concentration is
In 6mol/L hydrochloric acid, disperse 25-35 minutes, then remove supernatant liquor after standing 0.8-1.2 hours, leave and take the precipitation of lower floor
Thing；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is SnO2、SiO2Or ZnO；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
TiO2、CaO、Al2O3Or ZrO2, obtain activated synthetic fluoromica powder；
（2）Prepare silver ammino solution；
（3）Silver mirror reaction
Using the silver ammino solution prepared, by silver mirror reaction, nanometer is coated on activated synthetic fluoromica powder
Metallic silver layer（Nano metal silver layer is coated on the second active layer）, nanometer metallic silver cladding synthetic fluoromica is made
Powder.
Above-mentioned steps（1-1）Roughening（Also known as roughening is handled）, it is the light corrosion by acid, makes synthetic fluoromica
Powder surface produces uniform break chemical bonds, preferably can be combined with active layer.Above-mentioned steps（1-2）Activation, be
To the activation process on synthetic fluoromica powder surface, by liquid-phase deposition technique, on synthetic fluoromica powder surface
Active layer is formed, the group of argent can more be combined by producing powder surface, nanometer metallic silver is combined more firm.Active layer
It is divided into two layers, wherein internal layer is generally SnO2、SiO2Or ZnO, pre- combination is primarily served, roughened artificial conjunction is assigned
Into the transition zone that fluorophologopite powder is a thin layer of；Outer layer is generally TiO2、CaO、Al2O3Or ZrO2, primarily serve and build chemical bond
Effect, assign roughened synthetic fluoromica powder surface active chemical bond, Nano Silver is preferably adsorbed
Above.
It is preferred that above-mentioned steps（1-1-1）In, the particle diameter of the synthetic fluoromica powder taken is less than 10 microns, or
20-80 microns, or 50-200 microns.
It is preferred that above-mentioned steps（1-1-2）In, sediment is washed and is dehydrated using following methods：Add into sediment
Enter 350-450 parts by weight of deionized water and be stirred, be then dehydrated with plate and frame filter press.Above-mentioned washing, the process being dehydrated can
Carry out once or repeat repeatedly.Also deionized water can use to be cleaned during being dehydrated with plate and frame filter press.Sheet frame
The filter cake obtained after filter press dehydration is required roughened synthetic fluoromica powder.It is preferred that what is obtained is roughened
The water content of synthetic fluoromica powder is 18-22%（Weight）.
Above-mentioned steps（1-2）In, using the first activating solution, by liquid-phase precipitation method in the golden cloud of roughened artificial synthesized fluorine
The first active layer is coated in female powder；Using the second activating solution, the second activation is coated on the first active layer by liquid-phase precipitation method
Layer.First activating solution can use SnCl4Solution, solution of sodium metasilicate through or ZnCl2Solution, the first active layer of formation is SnO2Layer,
SiO2Layer or ZnO layer.Second activating solution can use TiCl4Solution, CaCl2Solution, AlCl3Solution or ZrCl4Solution, the of formation
Two active layers are TiO2Layer, CaO layers, Al2O3Layer or ZrO2Layer.
In a kind of preferred scheme, step（1-2-1）In by following techniques on roughened synthetic fluoromica powder
Coat the first active layer：（1-2-1-1）Roughened synthetic fluoromica powder is added in activating container, and to activation
250-350 parts by weight of deionized water is added in container, warming while stirring obtains feed liquid to 60-70 DEG C；Then kept in feed liquid
In the case of 60-70 DEG C of temperature, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）
The pH value of feed liquid is adjusted to 1.5-1.8；（1-2-1-2）Under conditions of feed temperature is 60-70 DEG C, by 80-120 parts by weight
Weight percent concentration is added drop-wise in feed liquid for 2.5% the first activating solution, is adjusted the pH value of feed liquid while adding pH adjusting agent
Between 1.5-1.8；First activating solution is SnCl4Solution.Preferred steps（1-2-1-2）In, with test solution membrane pump by
One activating solution（That is SnCl4Solution）Progressively it is added drop-wise in feed liquid, completed to be added dropwise in 0.8-1.2 hours.
In another preferred scheme, step（1-2-1）In by following techniques in roughened synthetic fluoromica powder
The first active layer of upper cladding：（1-2-1-1）Roughened synthetic fluoromica powder is added in activating container, and to work
Change and 250-350 parts by weight of deionized water is added in container, warming while stirring obtains feed liquid to 80-85 DEG C；Then protected in feed liquid
In the case of the temperature for holding 80-85 DEG C, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（As concentration is molten for 10% NaOH
Liquid）The pH value of feed liquid is adjusted to 8.5-9.0；（1-2-1-2）Under conditions of feed temperature is 80-85 DEG C, by 20-30 weight
Part concentration is added drop-wise in feed liquid for 1mol/L the first activating solution, is adjusted the pH value of feed liquid in 8.5- while adding pH adjusting agent
9.0 between；First activating solution is solution of sodium metasilicate through.Preferred steps（1-2-1-2）In, first is lived with test solution membrane pump
Change liquid（That is solution of sodium metasilicate through）Progressively it is added drop-wise in feed liquid, completed to be added dropwise in 0.8-1.2 hours.
In another preferred scheme, step（1-2-1）In by following techniques in roughened synthetic fluoromica powder
The first active layer of upper cladding：（1-2-1-1）Roughened synthetic fluoromica powder is added in activating container, and to work
Change and 250-350 parts by weight of deionized water is added in container, warming while stirring obtains feed liquid to 80-85 DEG C；Then protected in feed liquid
In the case of the temperature for holding 80-85 DEG C, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（Such as the salt that concentration is 6mol/L
Acid）The pH value of feed liquid is adjusted to 5.0-6.0；（1-2-1-2）Under conditions of feed temperature is 80-85 DEG C, by 80-120 weights
Amount part weight percent concentration is added drop-wise in feed liquid for 2.0% the first activating solution, while adding pH adjusting agent by the pH value of feed liquid
Regulation is between 5.0-6.0；First activating solution is ZnCl2Solution.Preferred steps（1-2-1-2）In, use test solution membrane pump
By the first activating solution（That is ZnCl2Solution）Progressively it is added drop-wise in feed liquid, completed to be added dropwise in 0.8-1.2 hours.
In a kind of preferred scheme, step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-
2-1）After first activating solution is added dropwise to complete, pH adjusting agent is added into activating container（Such as the NaOH that weight percent concentration is 10%
Solution）, the pH value of feed liquid is adjusted to 2.0-2.2, while by the temperature adjustment of feed liquid to 75-85 DEG C；（1-2-2-2）In pH controls
Under the regulation of device processed, while adding second activating solution and pH adjusting agent of the concentration for 4mol/L into activating container（Such as weight hundred
Divide the NaOH solution that specific concentration is 10%）, and the pH value of feed liquid is maintained between 2.0-2.2；When the second activating solution of addition
When reaching 75-85 parts by weight, stop adding the second activating solution and pH adjusting agent；Then 75-85 DEG C of temperature is kept in feed liquid
In the case of to feed liquid stir 25-35 minute, then to feed liquid dehydration after obtain activated synthetic fluoromica powder；It is described
Second activating solution is TiCl4Solution.
More preferably step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press, needed for obtained filter cake is
Activated synthetic fluoromica powder.Deionized water also can use to carry out clearly during being dehydrated with plate and frame filter press
Wash.The water content of activated synthetic fluoromica powder is usually 18-22%.
More preferably step（1-2-2-2）In, while being pumped into the second activating solution and pH into activating container with test solution membrane pump
Conditioning agent, is pumped into speed by the control of pH controllers, pH value is maintained between 2.0-2.2.Above-mentioned pH controllers are as a tune
Control switch, it connects three lines；Wherein one line connects the pH value in pH electrodes, sensing solution, and current pH is shown in digital display screen
Value；Another two lines connect two test solution membrane pumps, and one is sour pole test solution membrane pump（TiCl4）, another be alkali pole test solution every
Membrane pump（NaOH）.Sour pole has been at addition state.PH value on pre-set digital display is in a scope（2.0-
2.2）, controller automatically opens up alkali pole pump when less than pH value, adds NaOH, pH value is increased, pH value is maintained into 2.0-2.2
Between.
In another preferred scheme, step（1-2-2）In the second active layer is coated on the first active layer by following techniques：
（1-2-2-1）After first activating solution is added dropwise to complete, pH adjusting agent is added into activating container（If weight percent concentration is 10%
NaOH solution or weight percent concentration be 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 11-12, while by the temperature of feed liquid
Degree regulation is to 60-70 DEG C；（1-2-2-2）Under the regulation of pH controllers, while it is 4mol/L that concentration is added into activating container
The second activating solution and pH adjusting agent（Such as the hydrochloric acid that weight percent concentration is 10%）, and the pH value of feed liquid is maintained at 11-
Between 12；When the second activating solution of addition reaches 40-50 parts by weight, stop adding the second activating solution and pH adjusting agent；Then
Feed liquid is stirred 25-35 minutes in the case where feed liquid keeps 60-70 DEG C of temperature, then to obtaining activated after feed liquid dehydration
Synthetic fluoromica powder；Second activating solution is CaCl2Solution.
More preferably step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press, needed for obtained filter cake is
Activated synthetic fluoromica powder.Deionized water also can use to carry out clearly during being dehydrated with plate and frame filter press
Wash.The water content of activated synthetic fluoromica powder is usually 18-22%.
More preferably step（1-2-2-2）In, while being pumped into the second activating solution and pH into activating container with test solution membrane pump
Conditioning agent, is pumped into speed by the control of pH controllers, pH value is maintained between 11-12.
In another preferred scheme, step（1-2-2）In the second active layer is coated on the first active layer by following techniques：
（1-2-2-1）After first activating solution is added dropwise to complete, pH adjusting agent is added into activating container（If weight percent concentration is 10%
NaOH solution or weight percent concentration be 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 9-10, while by the temperature of feed liquid
Degree regulation is to 80-85 DEG C；（1-2-2-2）Under the regulation of pH controllers, while it is 4mol/L that concentration is added into activating container
The second activating solution and pH adjusting agent（Such as the hydrochloric acid that weight percent concentration is 10%）, and the pH value of feed liquid is maintained at 9-
Between 10；When the second activating solution of addition reaches 50-60 parts by weight, stop adding the second activating solution and pH adjusting agent；Then
Feed liquid is stirred 25-35 minutes in the case where feed liquid keeps 80-85 DEG C of temperature, then to obtaining activated after feed liquid dehydration
Synthetic fluoromica powder；Second activating solution is AlCl3Solution.
More preferably step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press, needed for obtained filter cake is
Activated synthetic fluoromica powder.Deionized water also can use to carry out clearly during being dehydrated with plate and frame filter press
Wash.The water content of activated synthetic fluoromica powder is usually 18-22%.
More preferably step（1-2-2-2）In, while being pumped into the second activating solution and pH into activating container with test solution membrane pump
Conditioning agent, is pumped into speed by the control of pH controllers, pH value is maintained between 9-10.
In another preferred scheme, step（1-2-2）In the second active layer is coated on the first active layer by following techniques：
（1-2-2-1）After first activating solution is added dropwise to complete, pH adjusting agent is added into activating container（If weight percent concentration is 10%
NaOH solution or weight percent concentration be 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 1.3-2.3, while by feed liquid
Temperature adjustment is to 75-85 DEG C；（1-2-2-2）Under the regulation of pH controllers, while it is 4mol/ that concentration is added into activating container
L the second activating solution and pH adjusting agent（Such as the NaOH solution that weight percent concentration is 10%）, and keep the pH value of feed liquid
Between 1.3-2.3；When the second activating solution of addition reaches 70-80 parts by weight, stop adding the second activating solution and pH regulations
Agent；Then feed liquid is stirred 25-35 minutes in the case of the temperature that 75-85 DEG C is kept in feed liquid, then to being obtained after feed liquid dehydration
Activated synthetic fluoromica powder；Second activating solution is ZrCl4Solution.
More preferably step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press, needed for obtained filter cake is
Activated synthetic fluoromica powder.Deionized water also can use to carry out clearly during being dehydrated with plate and frame filter press
Wash.The water content of activated synthetic fluoromica powder is usually 18-22%.
More preferably step（1-2-2-2）In, while being pumped into the second activating solution and pH into activating container with test solution membrane pump
Conditioning agent, is pumped into speed by the control of pH controllers, pH value is maintained between 1.3-2.3.
Preferred steps（2）In, the method for preparing silver ammino solution is：By 12-16 parts by weight AgNO3 With 200-300 parts by weight weights
Amount percent concentration is mixed and stirred for uniformly for 5% NaOH solution, and the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise,
To solution clarification, then the nitre acid for adjusting pH value for being 15-16% with weight percent concentration silver ammino solution is obtained to 12-13.Silver-colored ammonia
Solution is generally now matched somebody with somebody in process of production.
Preferred steps（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
250-350 parts by weight of deionized water is added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, then added
Enter 0.04-0.06 parts by weight sodium thiosulfate, stir 0.8-1.2 hours（The purpose of stirring is to make sodium thiosulfate fully molten
Solution, and synthetic fluoromica powder is uniformly dispersed in deionized water）；
（3-2）Reducing solution is gradually added into reaction vessel, addition is completed in 1-2 hours, then stirs 0.8-1.2 small
When, then the pH value of material in reaction vessel is adjusted to 12-13；
Reducing solution used is prepared by following techniques：Take the anhydrous acetaldehyde of 7-9 parts by weight, 200-280 parts by weight percentage by weights dense
The ethanol solution mixing for 30% is spent, reducing solution is obtained after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring（Mixing speed can be
250-350rpm）, silver ammino solution addition completion in 0.8-1.2 hours（The adding speed of silver ammino solution is controlled in 5ml/min
Left and right）；During silver ammino solution is added, the temperature of charge control in reaction vessel is adjusted at 20-30 DEG C, and with nitric acid
The pH value of material in reaction vessel is saved, the pH value of material in reaction vessel is maintained 12-13；
（3-4）Add after silver ammino solution, insulated and stirred 0.8-1.2 hours（Mixing speed can be 250-350rpm）, then filter
Go out powder and dried, obtain nanometer metallic silver cladding synthetic fluoromica powder.
Above-mentioned steps（3）The equation of reaction is：
R-CHO+2Ag(NH3)2OH→R-COONH4+H2O+2Ag↓+3NH3。
Above-mentioned steps（3）From reducing process in activated synthetic fluoromica powder coated with silver on surface, i.e., in solution
The reducing agent of middle addition can provide electronics after being oxidized, precipitate reduction goes out argent and coats activated synthetic fluoromica
Powder.The technique of coated with silver is similarly liquid phase deposition, and its key problem in technology is：First, the artificial synthesized fluorine gold being wrapped by is made
Mica powder is evenly spread in liquid；Secondly, the process conditions by controlling to coat（Include the grain of synthetic fluoromica powder
Degree, concentration, the pH value of solution coat temperature and time of process etc.）, to realize that it is activated that nanometer metallic silver is evenly coated at
On synthetic fluoromica powder.
It is adapted to the material of configuration reducing solution（Solute）The material of aldehyde radical can also be possessed using formaldehyde, sodium potassium tartrate tetrahydrate etc..
Above-mentioned steps（1-1-1）Synthetic fluoromica powder used is commercially available.
Preferred steps（1-1-1）Synthetic fluoromica powder used is obtained by following techniques：
（1-1-1-1）Synthetic mica piece after fluffy, operating procedure is as follows：The first step, synthetic fluoromica piece is put into
In electric furnace, boil 3 hours；Second step, synthetic fluoromica piece is taken out, in input cold water, by expanding with heat and contract with cold
Process, make piece expanded in advance；3rd step, configures a certain amount of sodium carbonate liquor, puts into the artificial synthesized fluorine anticipated
Phlogopite piece, soaks 24 hours at room temperature；4th step, the synthetic fluoromica piece for soaking sodium carbonate is put into certain dense
The ammonium chloride solution of degree, soaks 1 hour；5th step, soaked synthetic fluoromica piece is taken out, 350 DEG C is inserted and forges
Burn, washing；
（1-1-1-2）Hydraulic fracture：Waterpower paper-making pulper is taken, synthetic fluoromica piece is slightly peeled off, passed through
The removal of impurities grading technology of ladder screen cloth, obtains pure synthetic fluoromica slurry；
（1-1-1-3）Delaminate grinding：Synthetic fluoromica slurry is ground, the powder crystal being ground should be made unilateral
Do not lost by mechanical force, again can be levigate by powder, reach and be maximally maintained unilateral smooth of powder, be conducive to follow-up
Cladding；
（1-1-1-4）Compound online classification：The powder that grinding is obtained is classified；
（1-1-1-5）Pneumatic dehydration.
Above-mentioned steps（1-1-1-1）Changed by the states of matter of chemical immersion synthetic fluoromica piece process, made artificial
The cleavage surface of synthesis fluorophologopite piece interlayer is effectively peeled off, and provides wet grinding good premise, its concrete operations can
A kind of referenced patent number " synthetic fluoromica piece disclosed in ZL201310355762.9 Chinese invention patent specification
The method of fluffy ".
Above-mentioned steps（1-1-1-4）Patent No. ZL201620503450.7 Chinese utility model patent specification can be used
Disclosed " compound mica is combined online grading plant " is carried out.
Above-mentioned steps（1-1-1-5）Patent No. ZL201620503454.5 Chinese utility model patent specification can be used
Disclosed " the pneumatic dehydration device of synthesis fluorophologopite powder " is carried out.Because the subsequent handling of pretreatment needs to add water, thus it is de-
The powder obtained after water need not be dried, and keep moisture in 18-22%.
Synthetic fluoromica powder has the advantages such as high-purity, high-weatherability, high tenacity, resistance to acids and bases, does not contain to human body
Harmful lead, mercury, arsenic element, and surfacing is smooth, in minute surface, nanometer metallic silver is coated on thereon, does not interfere with argent
The performance of itself（Such as electrical and thermal conductivity）；Outside synthetic fluoromica powder coat one layer of nano level metal silver, by its from
Insulating materials is changed into conductive material, while the properties such as its silver-colored argent gloss, special catalytic property are assigned, in conjunction with
The properties such as high intensity, high tenacity, the good weatherability of synthetic fluoromica powder so that the feature of the composite granule is strong.Letter
For it, nanometer metallic silver produced by the present invention cladding synthetic fluoromica powder has good conductive and heat-conductive catalytic
The premium properties such as energy, excellent decoration performance, high intensity, high tenacity, good chemical resistance, nontoxic free from admixture, quality be light, and cost
Cheap, cost performance is high, is conducive to widening its application in many technical fields.
Nanometer metallic silver produced by the present invention cladding synthetic fluoromica powder can be widely applied to aerospace industry,
The fields such as daily anti-corrosion, daily decoration, organic chemical industry, marine paint, the antistatic process in high-end electronic field, can lower visitor
Family use cost.
Embodiment
Embodiment 1
The preparation method of nanometer metallic silver cladding synthetic fluoromica powder comprises the steps in the present embodiment：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）Take 100 parts by weight synthetic fluoromica powder（By dry weight）, 400 parts by weight concentration are added to for 6mol/
In L hydrochloric acid, disperse 30 minutes, then remove supernatant liquor after standing 1 hour, leave and take the sediment of lower floor；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
This step（1-1-2）In, sediment is washed and is dehydrated using following methods：400 weight are added into sediment
Part deionized water is simultaneously stirred, and is then dehydrated with plate and frame filter press（It can also be spent during being dehydrated with plate and frame filter press
Ionized water is cleaned）；The filter cake obtained after plate and frame filter press dehydration is required roughened synthetic fluoromica
Powder（The water content of obtained roughened synthetic fluoromica powder is 18-22%（Weight））；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is SnO2；
This step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-
2-1-1）Roughened synthetic fluoromica powder is added in activating container, and adds into activating container 300 weight
Part deionized water, warming while stirring obtains feed liquid to 60-70 DEG C；Then the situation of 60-70 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 30 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）The pH value of feed liquid is adjusted to 1.5-
1.8；（1-2-1-2）It is with test solution membrane pump that 100 parts by weight percentage by weights are dense under conditions of feed temperature is 60-70 DEG C
Spend the first activating solution for 2.5%（First activating solution is SnCl4Solution）Progressively it is added drop-wise in feed liquid, while adding pH adjusting agent
The pH value of feed liquid is adjusted between 1.5-1.8, completed to be added dropwise in 1 hour；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
TiO2, obtain activated synthetic fluoromica powder；
This step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution
After being added dropwise to complete, pH adjusting agent is added into activating container（Such as the NaOH solution that weight percent concentration is 10%）, by feed liquid
PH value is adjusted to 2.0-2.2, while by the temperature adjustment of feed liquid to 75-85 DEG C；（1-2-2-2）Under the regulation of pH controllers,
The second activating solution that concentration is 4mol/L is added into activating container simultaneously（Second activating solution is TiCl4Solution）And pH adjusting agent
（Such as the NaOH solution that weight percent concentration is 10%）, and the pH value of feed liquid is maintained between 2.0-2.2；When addition
When second activating solution reaches 80 parts by weight, stop adding the second activating solution and pH adjusting agent；Then kept for 75-85 DEG C in feed liquid
Feed liquid is stirred 30 minutes in the case of temperature, then to obtaining activated synthetic fluoromica powder after feed liquid dehydration；
Step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press（During being dehydrated with plate and frame filter press also
It can be cleaned with deionized water）, obtained filter cake is required activated synthetic fluoromica powder；Activated
The water content of synthetic fluoromica powder is usually 18-22%；
Step（1-2-2-2）In, while being pumped into the second activating solution and pH adjusting agent into activating container with test solution membrane pump, pass through
The control of pH controllers is pumped into speed, pH value is maintained between 2.0-2.2；
（2）Prepare silver ammino solution；
This step（2）In, the method for preparing silver ammino solution is：By 14 parts by weight AgNO3 It is dense with 250 parts by weight percentage by weights
The NaOH solution spent for 5% is mixed and stirred for uniformly, and the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise, clear to solution
Clearly, then with the nitre acid for adjusting pH value that weight percent concentration is 15.5% to 12.5, silver ammino solution is obtained；
（3）Silver mirror reaction
This step（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
300 parts by weight of deionized water are added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, added
0.05 parts by weight sodium thiosulfate, is stirred 1 hour；
（3-2）Reducing solution is gradually added into reaction vessel, added completing in 1.5 hours, then stirs 1 hour, then will
The pH value of material is adjusted to 12-13 in reaction vessel；
Reducing solution used is prepared by following techniques：It is 30% to take the anhydrous acetaldehyde of 8 parts by weight, 242 parts by weight weight percent concentrations
Ethanol solution mixing, obtain reducing solution after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring（Mixing speed is
300rpm）, silver ammino solution added completion in 1 hour（The adding speed of silver ammino solution is controlled in 5ml/min or so）；In addition
During silver ammino solution, the temperature of charge in reaction vessel is controlled at 20-30 DEG C, and adjusted with nitric acid in reaction vessel
The pH value of material, makes the pH value of material in reaction vessel maintain 12-13；
（3-4）Add after silver ammino solution, insulated and stirred 1 hour（Mixing speed is 300rpm）, then filter out powder and carry out
Drying, obtains nanometer metallic silver cladding synthetic fluoromica powder（By above-mentioned silver mirror reaction, activated artificial synthesized
Nano metal silver layer is coated on fluorophologopite powder）.
Embodiment 2
The preparation method of nanometer metallic silver cladding synthetic fluoromica powder comprises the steps in the present embodiment：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）Take 100 parts by weight synthetic fluoromica powder（By dry weight）, 480 parts by weight concentration are added to for 6mol/
In L hydrochloric acid, disperse 25 minutes, then remove supernatant liquor after standing 0.8 hour, leave and take the sediment of lower floor；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
This step（1-1-2）In, sediment is washed and is dehydrated using following methods：420 weight are added into sediment
Part deionized water is simultaneously stirred, and is then dehydrated with plate and frame filter press（It can also be spent during being dehydrated with plate and frame filter press
Ionized water is cleaned）；The filter cake obtained after plate and frame filter press dehydration is required roughened synthetic fluoromica
Powder（The water content of obtained roughened synthetic fluoromica powder is 18-22%（Weight））；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is SiO2；
This step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-
2-1-1）Roughened synthetic fluoromica powder is added in activating container, and adds into activating container 350 weight
Part deionized water, warming while stirring obtains feed liquid to 80-85 DEG C；Then the situation of 80-85 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 25 minutes；PH adjusting agent is used again（Such as the NaOH solution that concentration is 10%）The pH value of feed liquid is adjusted to 8.5-
9.0；（1-2-1-2）It by 30 parts by weight concentration is 1mol/L's with test solution membrane pump under conditions of 80-85 DEG C to be in feed temperature
First activating solution（First activating solution is solution of sodium metasilicate through）Progressively it is added drop-wise in feed liquid, while adding pH adjusting agent by feed liquid
PH value is adjusted between 8.5-9.0, completes to be added dropwise in 1.2 hours；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
CaO, obtains activated synthetic fluoromica powder；
This step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution
After being added dropwise to complete, pH adjusting agent is added into activating container（Such as the NaOH solution or weight percent that weight percent concentration is 10%
Specific concentration is 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 11-12, while by the temperature adjustment of feed liquid to 60-70 DEG C；（1-
2-2-2）Under the regulation of pH controllers, while adding the second activating solution that concentration is 4mol/L into activating container（Second lives
It is CaCl to change liquid2Solution）And pH adjusting agent（Such as the hydrochloric acid that weight percent concentration is 10%）, and keep the pH value of feed liquid
Between 11-12；When the second activating solution of addition reaches 50 parts by weight, stop adding the second activating solution and pH adjusting agent；So
Feed liquid is stirred 35 minutes in the case of the temperature for keeping 60-70 DEG C in feed liquid afterwards, then to obtaining activated after feed liquid dehydration
Synthetic fluoromica powder；
Step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press（During being dehydrated with plate and frame filter press also
It can be cleaned with deionized water）, obtained filter cake is required activated synthetic fluoromica powder；Activated
The water content of synthetic fluoromica powder is usually 18-22%；
Step（1-2-2-2）In, while being pumped into the second activating solution and pH adjusting agent into activating container with test solution membrane pump, pass through
The control of pH controllers is pumped into speed, pH value is maintained between 11-12；
（2）Prepare silver ammino solution；
This step（2）In, the method for preparing silver ammino solution is：By 12 parts by weight AgNO3 It is dense with 300 parts by weight percentage by weights
The NaOH solution spent for 5% is mixed and stirred for uniformly, and the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise, clear to solution
Clearly, then with the nitre acid for adjusting pH value that weight percent concentration is 15% to 12-13, silver ammino solution is obtained；
（3）Silver mirror reaction
This step（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
250 parts by weight of deionized water are added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, added
0.04 parts by weight sodium thiosulfate, is stirred 0.8 hour；
（3-2）Reducing solution is gradually added into reaction vessel, added completing in 2 hours, then stirs 0.8 hour, then will
The pH value of material is adjusted to 12-13 in reaction vessel；
Reducing solution used is prepared by following techniques：It is 30% to take the anhydrous acetaldehyde of 9 parts by weight, 280 parts by weight weight percent concentrations
Ethanol solution mixing, obtain reducing solution after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring（Mixing speed is
250rpm）, silver ammino solution added completion in 1.2 hours（The adding speed of silver ammino solution is controlled in 5ml/min or so）；
During adding silver ammino solution, the temperature of charge in reaction vessel is controlled at 20-30 DEG C, and held with nitric acid regulation reaction
The pH value of material in device, makes the pH value of material in reaction vessel maintain 12-13；
（3-4）Add after silver ammino solution, insulated and stirred 1.2 hours（Mixing speed is 250rpm）, then filter out powder and go forward side by side
Row drying, obtains nanometer metallic silver cladding synthetic fluoromica powder（By above-mentioned silver mirror reaction, in activated artificial conjunction
Nano metal silver layer is coated on into fluorophologopite powder）.
Embodiment 3
The preparation method of nanometer metallic silver cladding synthetic fluoromica powder comprises the steps in the present embodiment：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）Take 100 parts by weight synthetic fluoromica powder（By dry weight）, 320 parts by weight concentration are added to for 6mol/
In L hydrochloric acid, disperse 35 minutes, then remove supernatant liquor after standing 1.2 hours, leave and take the sediment of lower floor；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
This step（1-1-2）In, sediment is washed and is dehydrated using following methods：350 weight are added into sediment
Part deionized water is simultaneously stirred, and is then dehydrated with plate and frame filter press（It can also be spent during being dehydrated with plate and frame filter press
Ionized water is cleaned）；The filter cake obtained after plate and frame filter press dehydration is required roughened synthetic fluoromica
Powder（The water content of obtained roughened synthetic fluoromica powder is 18-22%（Weight））；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is ZnO；
This step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-
2-1-1）Roughened synthetic fluoromica powder is added in activating container, and adds into activating container 280 weight
Part deionized water, warming while stirring obtains feed liquid to 80-85 DEG C；Then the situation of 80-85 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 28 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）The pH value of feed liquid is adjusted to 5.0-
6.0；（1-2-1-2）It is under conditions of 80-85 DEG C, with test solution membrane pump by 80-120 parts by weight percentage by weights in feed temperature
Concentration is 2.0% the first activating solution（First activating solution is ZnCl2Solution）Progressively it is added drop-wise in feed liquid, while adding pH regulations
Agent adjusts the pH value of feed liquid between 5.0-6.0, completes to be added dropwise in 1 hour；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
ZrO2, obtain activated synthetic fluoromica powder；
This step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution
After being added dropwise to complete, pH adjusting agent is added into activating container（Such as the NaOH solution or weight percent that weight percent concentration is 10%
Specific concentration is 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 1.3-2.3, while by the temperature adjustment of feed liquid to 75-85 DEG C；
（1-2-2-2）Under the regulation of pH controllers, while adding the second activating solution that concentration is 4mol/L into activating container（Second
Activating solution is ZrCl4Solution）And pH adjusting agent（Such as the NaOH solution that weight percent concentration is 10%）, and make the pH of feed liquid
Value is maintained between 1.3-2.3；When the second activating solution of addition reaches 70 parts by weight, stop adding the second activating solution and pH is adjusted
Save agent；Then feed liquid is stirred 32 minutes in the case of the temperature that 75-85 DEG C is kept in feed liquid, then to being obtained after feed liquid dehydration
Activated synthetic fluoromica powder；
This step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press（During being dehydrated with plate and frame filter press
Also deionized water can use to be cleaned）, obtained filter cake is required activated synthetic fluoromica powder；It is activated
The water content of synthetic fluoromica powder be usually 18-22%；
This step（1-2-2-2）In, while being pumped into the second activating solution and pH adjusting agent into activating container with test solution membrane pump, lead to
Cross the control of pH controllers and be pumped into speed, pH value is maintained between 1.3-2.3；
（2）Prepare silver ammino solution；
This step（2）In, the method for preparing silver ammino solution is：By 16 parts by weight AgNO3 It is dense with 270 parts by weight percentage by weights
The NaOH solution spent for 5% is mixed and stirred for uniformly, and the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise, clear to solution
Clearly, then with the nitre acid for adjusting pH value that weight percent concentration is 16% to 12-13, silver ammino solution is obtained；
（3）Silver mirror reaction
This step（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
350 parts by weight of deionized water are added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, added
0.06 parts by weight sodium thiosulfate, is stirred 1.2 hours（The purpose of stirring is sodium thiosulfate is fully dissolved, and makes artificial conjunction
It is uniformly dispersed in deionized water into fluorophologopite powder）；
（3-2）Reducing solution is gradually added into reaction vessel, added completing in 1 hour, then stirs 1.2 hours, then will
The pH value of material is adjusted to 12-13 in reaction vessel；
Reducing solution used is prepared by following techniques：It is 30% to take the anhydrous acetaldehyde of 7 parts by weight, 200 parts by weight weight percent concentrations
Ethanol solution mixing, obtain reducing solution after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring（Mixing speed is
350rpm）, silver ammino solution added completion in 0.8 hour（The adding speed of silver ammino solution is controlled in 5ml/min or so）；Adding
Plus during silver ammino solution, the temperature of charge in reaction vessel is controlled at 20-30 DEG C, and adjust reaction vessel with nitric acid
The pH value of middle material, makes the pH value of material in reaction vessel maintain 12-13；
（3-4）Add after silver ammino solution, insulated and stirred 0.8 hour（Mixing speed is 350rpm）, then filter out powder and go forward side by side
Row drying, obtains nanometer metallic silver cladding synthetic fluoromica powder（By above-mentioned silver mirror reaction, in activated artificial conjunction
Nano metal silver layer is coated on into fluorophologopite powder）.
Embodiment 4
The preparation method of nanometer metallic silver cladding synthetic fluoromica powder comprises the steps in the present embodiment：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）Take 100 parts by weight synthetic fluoromica powder（By dry weight）, 420 parts by weight concentration are added to for 6mol/
In L hydrochloric acid, disperse 32 minutes, then remove supernatant liquor after standing 0.9 hour, leave and take the sediment of lower floor；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
This step（1-1-2）In, sediment is washed and is dehydrated using following methods：450 weight are added into sediment
Part deionized water is simultaneously stirred, and is then dehydrated with plate and frame filter press（It can also be spent during being dehydrated with plate and frame filter press
Ionized water is cleaned）；The filter cake obtained after plate and frame filter press dehydration is required roughened synthetic fluoromica
Powder（The water content of obtained roughened synthetic fluoromica powder is 18-22%（Weight））；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is SnO2；
This step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-
2-1-1）Roughened synthetic fluoromica powder is added in activating container, and adds into activating container 320 weight
Part deionized water, warming while stirring obtains feed liquid to 60-70 DEG C；Then the situation of 60-70 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 32 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）The pH value of feed liquid is adjusted to 1.5-
1.8；（1-2-1-2）It is under conditions of 60-70 DEG C, with test solution membrane pump by 90 parts by weight weight percent concentrations in feed temperature
For 2.5% the first activating solution（First activating solution is SnCl4Solution）Progressively it is added drop-wise in feed liquid, will while adding pH adjusting agent
The pH value of feed liquid is adjusted between 1.5-1.8, completes to be added dropwise in 1.1 hours；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
Al2O3, obtain activated synthetic fluoromica powder；
This step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution
After being added dropwise to complete, pH adjusting agent is added into activating container（Such as the NaOH solution or weight percent that weight percent concentration is 10%
Specific concentration is 10% hydrochloric acid）, the pH value of feed liquid is adjusted to 9-10, while by the temperature adjustment of feed liquid to 80-85 DEG C；（1-2-
2-2）Under the regulation of pH controllers, while adding the second activating solution that concentration is 4mol/L into activating container（Second activation
Liquid is AlCl3Solution）And pH adjusting agent（Such as the hydrochloric acid that weight percent concentration is 10%）, and it is maintained at the pH value of feed liquid
Between 9-10；When the second activating solution of addition reaches 55 parts by weight, stop adding the second activating solution and pH adjusting agent；Then exist
Feed liquid keeps stirring feed liquid 30 minutes in the case of 80-85 DEG C of temperature, then obtains activated artificial after being dehydrated to feed liquid
Synthesize fluorophologopite powder；
Step（1-2-2-2）In, feed liquid is dehydrated using plate and frame filter press（During being dehydrated with plate and frame filter press also
It can be cleaned with deionized water）, obtained filter cake is required activated synthetic fluoromica powder；Activated
The water content of synthetic fluoromica powder is usually 18-22%；
Step（1-2-2-2）In, while being pumped into the second activating solution and pH adjusting agent into activating container with test solution membrane pump, pass through
The control of pH controllers is pumped into speed, pH value is maintained between 9-10；
（2）Prepare silver ammino solution；
This step（2）In, the method for preparing silver ammino solution is：By 15 parts by weight AgNO3 It is dense with 200 parts by weight percentage by weights
The NaOH solution spent for 5% is mixed and stirred for uniformly, and the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise, clear to solution
Clearly, then with the nitre acid for adjusting pH value that weight percent concentration is 15% to 12-13, silver ammino solution is obtained；
（3）Silver mirror reaction
This step（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
300 parts by weight of deionized water are added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, added
0.045 parts by weight sodium thiosulfate, is stirred 1 hour；
（3-2）Reducing solution is gradually added into reaction vessel, added completing in 1.5 hours, then stirs 0.9 hour, then
The pH value of material in reaction vessel is adjusted to 12-13；
Reducing solution used is prepared by following techniques：It is 30% to take the anhydrous acetaldehyde of 8 parts by weight, 250 parts by weight weight percent concentrations
Ethanol solution mixing, obtain reducing solution after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring（Mixing speed is
300rpm）, silver ammino solution added completion in 1 hour（The adding speed of silver ammino solution is controlled in 5ml/min or so）；In addition
During silver ammino solution, the temperature of charge in reaction vessel is controlled at 20-30 DEG C, and adjusted with nitric acid in reaction vessel
The pH value of material, makes the pH value of material in reaction vessel maintain 12-13；
（3-4）Add after silver ammino solution, insulated and stirred 1 hour（Mixing speed is 300rpm）, then filter out powder and carry out
Drying, obtains nanometer metallic silver cladding synthetic fluoromica powder（By above-mentioned silver mirror reaction, activated artificial synthesized
Nano metal silver layer is coated on fluorophologopite powder）.
The step of above-described embodiment 1-4（1-1-1）In, the particle diameter of the synthetic fluoromica powder taken is less than 10 microns,
Or 20-80 microns, or 50-200 microns, it is commercially available.
In addition, above-described embodiment 1-4 gives four kinds of examples of active layer composition, but the present invention is not limited to above implementation
Example, that is to say, that the first active layer of any one chemical composition（SnO2Layer, SiO2Layer or ZnO layer）All can be with any one change
The second active layer studied point（TiO2Layer, CaO layers, Al2O3Layer or ZrO2Layer）With reference to and constitute active layer, only need to activation step
From corresponding first activating solution, the second activating solution in rapid.
Claims (10)
1. a kind of nanometer metallic silver coats the preparation method of synthetic fluoromica powder, it is characterised in that comprise the steps：
（1）The pretreatment of synthetic fluoromica powder
（1-1）Roughening
（1-1-1）100 parts by weight synthetic fluoromica powder are taken, the salt that 320-480 parts by weight concentration is 6mol/L is added to
In acid, disperse 25-35 minutes, then remove supernatant liquor after standing 0.8-1.2 hours, leave and take the sediment of lower floor；
（1-1-2）With water by step（1-1-1）Obtained sediment is washed and is dehydrated, and obtains roughened artificial synthesized fluorine
Phlogopite powder；
（1-2）Activation
（1-2-1）The first active layer, the first activation are coated on roughened synthetic fluoromica powder with liquid-phase precipitation method
The chemical composition of layer is SnO2、SiO2Or ZnO；
（1-2-2）The second active layer is coated on the first active layer with liquid-phase precipitation method, the chemical composition of the second active layer is
TiO2、CaO、Al2O3Or ZrO2, obtain activated synthetic fluoromica powder；
（2）Prepare silver ammino solution；
（3）Silver mirror reaction
Using the silver ammino solution prepared, by silver mirror reaction, nanometer is coated on activated synthetic fluoromica powder
Metallic silver layer, is made nanometer metallic silver cladding synthetic fluoromica powder.
2. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-2-1-
1）Roughened synthetic fluoromica powder is added in activating container, and the addition 250-350 weight into activating container
Part deionized water, warming while stirring obtains feed liquid to 60-70 DEG C；Then the situation of 60-70 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）By the pH value of feed liquid adjust to
1.5-1.8；（1-2-1-2）Under conditions of feed temperature is 60-70 DEG C, it is by 80-120 parts by weight weight percent concentrations
2.5% the first activating solution is added drop-wise in feed liquid, is adjusted the pH value of feed liquid between 1.5-1.8 while adding pH adjusting agent；Institute
It is SnCl to state the first activating solution4Solution.
3. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-2-1-
1）Roughened synthetic fluoromica powder is added in activating container, and the addition 250-350 weight into activating container
Part deionized water, warming while stirring obtains feed liquid to 80-85 DEG C；Then the situation of 80-85 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（Such as the NaOH solution that concentration is 10%）By the pH value of feed liquid adjust to
8.5-9.0；（1-2-1-2）It is the first of 1mol/L by 20-30 parts by weight concentration under conditions of feed temperature is 80-85 DEG C
Activating solution is added drop-wise in feed liquid, is adjusted the pH value of feed liquid between 8.5-9.0 while adding pH adjusting agent；First activation
Liquid is solution of sodium metasilicate through.
4. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-1）In coat the first active layer on roughened synthetic fluoromica powder by following techniques：（1-2-1-
1）Roughened synthetic fluoromica powder is added in activating container, and the addition 250-350 weight into activating container
Part deionized water, warming while stirring obtains feed liquid to 80-85 DEG C；Then the situation of 80-85 DEG C of temperature is kept in feed liquid
Under, feed liquid is stirred 25-35 minutes；PH adjusting agent is used again（Such as the hydrochloric acid that concentration is 6mol/L）By the pH value of feed liquid adjust to
5.0-6.0；（1-2-1-2）Under conditions of feed temperature is 80-85 DEG C, it is by 80-120 parts by weight weight percent concentrations
2.0% the first activating solution is added drop-wise in feed liquid, is adjusted the pH value of feed liquid between 5.0-6.0 while adding pH adjusting agent；Institute
It is ZnCl to state the first activating solution2Solution.
5. the nanometer metallic silver according to claim any one of 2-4 coats the preparation method of synthetic fluoromica powder,
It is characterized in that step（1-2-1-2）In, the first activating solution is progressively added drop-wise in feed liquid with test solution membrane pump, in 0.8-1.2
Complete to be added dropwise in hour.
6. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution is added dropwise
After the completion of, pH adjusting agent is added into activating container, the pH value of feed liquid is adjusted to 2.0-2.2, while the temperature of feed liquid is adjusted
Section is to 75-85 DEG C；（1-2-2-2）Under the regulation of pH controllers, while it is the of 4mol/L that concentration is added into activating container
Two activating solutions and pH adjusting agent, and the pH value of feed liquid is maintained between 2.0-2.2；When the second activating solution of addition reaches
During 75-85 parts by weight, stop adding the second activating solution and pH adjusting agent；Then the situation of 75-85 DEG C of temperature is kept in feed liquid
Under to feed liquid stir 25-35 minute, then to feed liquid dehydration after obtain activated synthetic fluoromica powder；Described second
Activating solution is TiCl4Solution.
7. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution is added dropwise
After the completion of, pH adjusting agent is added into activating container, the pH value of feed liquid is adjusted to 11-12, while by the temperature adjustment of feed liquid
To 60-70 DEG C；（1-2-2-2）Under the regulation of pH controllers, while adding second that concentration is 4mol/L into activating container
Activating solution and pH adjusting agent, and the pH value of feed liquid is maintained between 11-12；When the second activating solution of addition reaches 40-50
During parts by weight, stop adding the second activating solution and pH adjusting agent；Then in the case where feed liquid keeps 60-70 DEG C of temperature to material
Liquid is stirred 25-35 minutes, then to obtaining activated synthetic fluoromica powder after feed liquid dehydration；Second activating solution
It is CaCl2Solution.
8. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution is added dropwise
After the completion of, pH adjusting agent is added into activating container, the pH value of feed liquid is adjusted to 9-10, while by the temperature adjustment of feed liquid extremely
80-85℃；（1-2-2-2）Under the regulation of pH controllers, while adding second work of the concentration for 4mol/L into activating container
Change liquid and pH adjusting agent, and the pH value of feed liquid is maintained between 9-10；When the second activating solution of addition reaches 50-60 weight
During part, stop adding the second activating solution and pH adjusting agent；Then feed liquid is stirred in the case of the temperature that 80-85 DEG C is kept in feed liquid
Mix 25-35 minutes, then to obtaining activated synthetic fluoromica powder after feed liquid dehydration；Second activating solution is
AlCl3Solution.
9. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In step（1-2-2）In the second active layer is coated on the first active layer by following techniques：（1-2-2-1）First activating solution is added dropwise
After the completion of, pH adjusting agent is added into activating container, the pH value of feed liquid is adjusted to 1.3-2.3, while the temperature of feed liquid is adjusted
Section is to 75-85 DEG C；（1-2-2-2）Under the regulation of pH controllers, while it is the of 4mol/L that concentration is added into activating container
Two activating solutions and pH adjusting agent, and the pH value of feed liquid is maintained between 1.3-2.3；When the second activating solution of addition reaches
During 70-80 parts by weight, stop adding the second activating solution and pH adjusting agent；Then the situation of 75-85 DEG C of temperature is kept in feed liquid
Under to feed liquid stir 25-35 minute, then to feed liquid dehydration after obtain activated synthetic fluoromica powder；Described second
Activating solution is ZrCl4Solution.
10. nanometer metallic silver according to claim 1 coats the preparation method of synthetic fluoromica powder, its feature exists
In：
Step（2）In, the method for preparing silver ammino solution is：By 12-16 parts by weight AgNO3 With 200-300 parts by weight weight percents
Specific concentration is mixed and stirred for uniformly for 5% NaOH solution, the ammoniacal liquor that weight percent concentration is 12.5% is then added dropwise, to solution
Clarification, then the nitre acid for adjusting pH value for being 15-16% with weight percent concentration obtain silver ammino solution to 12-13；
Step（3）The process of middle silver mirror reaction is：
（3-1）By step（1-2）The activated synthetic fluoromica powder obtained is added in reaction vessel, then to reaction
250-350 parts by weight of deionized water is added in container；Then the temperature of charge in reaction vessel is adjusted to 20-30 DEG C, then added
Enter 0.04-0.06 parts by weight sodium thiosulfate, stir 0.8-1.2 hours；
（3-2）Reducing solution is gradually added into reaction vessel, addition is completed in 1-2 hours, then stirs 0.8-1.2 small
When, then the pH value of material in reaction vessel is adjusted to 12-13；
Reducing solution used is prepared by following techniques：Take the anhydrous acetaldehyde of 7-9 parts by weight, 200-280 parts by weight percentage by weights dense
The ethanol solution mixing for 30% is spent, reducing solution is obtained after stirring；
（3-3）The silver ammino solution prepared is added gradually in reaction vessel in the case of stirring, silver ammino solution is in 0.8-
Add and complete in 1.2 hours；During silver ammino solution is added, the temperature of charge in reaction vessel is controlled in 20-30
DEG C, and with the pH value of material in nitric acid regulation reaction vessel, the pH value of material in reaction vessel is maintained 12-13；
（3-4）Add after silver ammino solution, then insulated and stirred 0.8-1.2 hours filters out powder and dried, received
Rice argent cladding synthetic fluoromica powder.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096795A (en) * | 2018-07-19 | 2018-12-28 | 安徽恒昊科技有限公司 | A kind of activation method of mica powder |
| CN109686498A (en) * | 2018-12-25 | 2019-04-26 | 深圳市欧科力科技有限公司 | A kind of preparation method of photoactive electrode slurry |
| CN113493209A (en) * | 2020-03-20 | 2021-10-12 | 广州昊吉生物科技有限公司 | Coating method of low-fluorine fluorophlogopite |
| CN115365495A (en) * | 2022-07-29 | 2022-11-22 | 广东三宝新材料科技股份有限公司 | Copper-coated mica powder and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61257479A (en) * | 1985-05-10 | 1986-11-14 | Agency Of Ind Science & Technol | Method for plating inorganic powder by electroless plating |
| JPH0224358A (en) * | 1988-07-14 | 1990-01-26 | Nippon Chem Ind Co Ltd | Polymer composition containing electrolessly plated powder |
| CN1919933A (en) * | 2006-09-01 | 2007-02-28 | 清华大学 | Method of preparing electric conductive adhesive by chemical plating silver on graphite powder surface |
| CN1974460A (en) * | 2006-12-01 | 2007-06-06 | 广东工业大学 | Silver plated hollow glass micro bead and its surface silver plating process |
| CN102212801A (en) * | 2011-05-25 | 2011-10-12 | 中北大学 | Chemical silvering method for PS (polystyrene) microspheres |
-
2017
- 2017-07-03 CN CN201710534173.5A patent/CN107130231B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61257479A (en) * | 1985-05-10 | 1986-11-14 | Agency Of Ind Science & Technol | Method for plating inorganic powder by electroless plating |
| JPH0224358A (en) * | 1988-07-14 | 1990-01-26 | Nippon Chem Ind Co Ltd | Polymer composition containing electrolessly plated powder |
| CN1919933A (en) * | 2006-09-01 | 2007-02-28 | 清华大学 | Method of preparing electric conductive adhesive by chemical plating silver on graphite powder surface |
| CN1974460A (en) * | 2006-12-01 | 2007-06-06 | 广东工业大学 | Silver plated hollow glass micro bead and its surface silver plating process |
| CN102212801A (en) * | 2011-05-25 | 2011-10-12 | 中北大学 | Chemical silvering method for PS (polystyrene) microspheres |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096795A (en) * | 2018-07-19 | 2018-12-28 | 安徽恒昊科技有限公司 | A kind of activation method of mica powder |
| CN109686498A (en) * | 2018-12-25 | 2019-04-26 | 深圳市欧科力科技有限公司 | A kind of preparation method of photoactive electrode slurry |
| CN113493209A (en) * | 2020-03-20 | 2021-10-12 | 广州昊吉生物科技有限公司 | Coating method of low-fluorine fluorophlogopite |
| CN115365495A (en) * | 2022-07-29 | 2022-11-22 | 广东三宝新材料科技股份有限公司 | Copper-coated mica powder and preparation method thereof |
| CN115365495B (en) * | 2022-07-29 | 2024-05-28 | 广东三宝新材料科技股份有限公司 | Copper-coated mica powder and preparation method thereof |
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